Catechol → 4-(2,2,2-Trichloro-1-hydroxyethyl)benzene-1,2-diol

온도

0 °C

To the solution of 440 g of 1,2-dihydroxybenzene dissolved in 1 L of methylene dichloride was added 1036 g of trichloroacetaldehyde monohydrate and then the reaction solution was cooled down to 0° C. 102 g of triethylamine was slowly added dropwise thereto. The reaction solution was warmed to room temperature, stirred for about 20 minutes, heated to 50° C. and then stirred for further 3 hours while maintaining the same temperature. After the reaction is completed, the reaction mixture was distilled under reduced pressure to remove methylene dichloride. The residue was dissolved in 4 L of ethylacetate, washed successively with 2400 ml of 0.5N-aqueous hydrochloric acid solution and 2 L of saturated saline, dried over anhydrous magnesium sulfate and then distilled under reduced pressure to remove the solvent and to obtain 540 g of the title compound.

1. temperatureThe reaction solution was warmed to room temperature
2. temperatureheated to 50° C.
3. stirringstirred for further 3 hours
4. temperaturewhile maintaining the same temperature
5. distillationthe reaction mixture was distilled under reduced pressure
6. customto remove methylene dichloride
7. dissolutionThe residue was dissolved in 4 L of ethylacetate
8. washwashed successively with 2400 ml of 0.5N-aqueous hydrochloric acid solution and 2 L of saturated saline
9. dry with materialdried over anhydrous magnesium sulfate
10. distillationdistilled under reduced pressure
11. customto remove the solvent

ORD 기록

ord-7f1f2144100f4a8e9624f9a6edc46410

출처 데이터셋

uspto-grants-1996_07

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US05541175